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The advances of adhesive den-tistry have an increasing

importance to the esthetic aspect ofdental care. Among tooth-coloredrestorative materials, ceramics andindirect composite resins can beused to replace partially or com-pletely metal-supported restorationsor even as inlays, onlays, laminatedveneers, and crowns.1

Ceramic materials have someimportant properties, such astranslucency,1–3 chemical stabil-ity,2,4 fluorescence,1,3–6 biocompat-ibility,1,4,7–9 a high resistance tocompression, and a coefficient ofthermal expansion similar to toothstructure,10,11 in spite of some clin-ical disadvantages and limitations,such as friability and susceptibility

to fracture propagation.3,9–11

Those properties indicate thatceramics are materials capable ofmimicking human enamel. Severalalternatives have been developedto increase their mechanical prop-erties and expand their clinicalapplications, based on the princi-ples of reinforcement with ceramicoxides, manufacturing technique,

*Professor at Department of Operative Dentistry and Dental Materials, Dentistry School, Federal Universityof Uberlândia, Uberlândia, MG, Brazil†Graduate student at Dentistry School, Federal University of Uberlândia, Uberlândia, MG, Brazil

Surface Treatment Protocols in the CementationProcess of Ceramic and Laboratory-Processed Composite Restorations: A Literature Review

CARLOS JOSÉ SOARES, DDS, MS, PHD*

PAULO VINICIUS SOARES, DDS†

JANAINA CARLA PEREIRA, DDS†

RODRIGO BORGES FONSECA, DDS, MS†

ABSTRACT

The clinical longevity of indirect restorations made of ceramics or indirect composite resinsdepends on their successful treatment and cementation. The cementation technique is determinedby the type of restorative material—ceramics or indirect composite resins; thus, their intaglio sur-face treatment should be performed according to their particular compositions. The aim of this lit-erature review was to define surface treatment protocols of different esthetic indirect restorativematerials. A PubMed database search was conducted for in vitro studies pertaining to the mostcommon treatment protocols of tooth-colored materials. Articles that described at least the surfacetreatment procedure, its effects on adhesion, its relationship with the material’s composition, clini-cal aspects, and expected longevity were selected. The search was limited to peer-reviewed articlespublished in English between 1965 and 2004 in dental journals. Sandblasting, etching techniques,and silane coupling agents are the most common procedures with improved results.

CLINICAL SIGNIFICANCE

Tooth-colored restorative materials vary considerably in composition and require different proto-cols for adhesive cementation.

(J Esthet Restor Dent 17:224–235, 2005)

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and improvement of adhesion todental structure.2,3,12–17

The use of feldspathic ceramic reinforced with a large amount of leucite,3,12,18,19 lithium di-silicate,1,3,20–23 aluminum oxide,and zirconium has resulted in betterfracture resistance.3,12,14,15,24–26

However, according to Borges andcolleagues, the clinical success ofceramic restorations depends on the cementation process, whichvaries according to the compositionof the ceramic material.1

As with the ceramic materials, com-posite resins also present satisfactorycharacteristics such translucence,surface polishing, resilience, andpositive esthetics.27 According toFerracane,28 direct composite resinshave limited indications becausethey present volumetric contractionduring the process of polymeriza-tion resulting in stress concentra-tion at the adhesive interface,29

cusp flexure,30 postoperative sensi-tivity,31 microleakage, and sec-ondary caries.31 In the face of thosedisadvantages, the first generationof laboratory-developed resins wasdeveloped in the early 1980s toovercome some of the inherent deficiencies of composite resins,including polymerization shrinkage,inadequate polymerization, andrestoration of proximal contactsand contour.32 In spite of this, thosematerials are characterized by asmall amount of inorganic micro-

fillers, presenting both low resis-tance against wear and undesirableclinical results.27 This situationstimulated the manufacturers, in theearly 1990s, to develop a secondgeneration of laboratory resins, lab-oratory-processed composite resins.These present a composition similarto that of current direct compositeresins,33 although they are processedby sophisticated techniques thatcombine heat, pressure, vacuum,and high light intensity.29,34

These new composite resins mightpresent either high amounts of fillercontent—such as Targis (Ivoclar,Schaan, Liechtenstein), Artglass(Heraeus Kulzer Inc., South Bend,IN, USA), and belleGlass (SDS-Kerr,Orange, CA, USA)—which makesthem adequate for restoring poste-rior teeth, or a intermediate fillervolume fraction, such as Solidex(Shofu Inc., Kyoto, Japan), enablingbetter esthetics. However, the smalleramount of inorganic particles in thislatter group makes them speciallyindicated for anterior teeth.27,33,35,36

The penetration of monomers intodemineralized dentinal structureafter polymerization promotes amicromechanical bond through the formation of a hybrid layer.37

The same principle of this retentionprocess can be similarly reproducedin the intaglio surface of ceramic or laboratory-processed compositeresin restorations through the useof different treatments. Depending

on the restorative material, this fact is based either on mechanicalbond obtained with aluminumoxide or diamond sandblasting, oron chemical bond, conferred by theapplication of a silane bondingagent or even with its inside struc-tural modification.3,12,38–42

The treatment of the intaglio sur-face of indirect restorations isdependent on the composition ofthe restorative material.1,33 In thepresence of a large amount of dif-ferent indirect restorative materialsshowing different composition andsurface treatment options, it seemsadequate to analyze the literature to look for methods that guide theclinician during the cementation of indirect restorations made ofceramics or indirect compositeresins, in an attempt to simplify aprocedure of such great importanceto clinical longevity of restorations.33

Therefore, the aim of this study wasto discuss the most common surfacetreatment protocols of differentindirect restorative materials bymeans of reviewing the literature.This literature review was based ona PubMed database search limitedto peer-reviewed articles in Englishthat were published between 1965and 2004 in dental journals. Thefollowing key words were used inthe PubMed search: “ceramic sur-face treatment,” “composite resinsurface treatment,” “ceramic andlaboratorial resin restorations,” and

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“silane surface treatment.” Articlesthat described at least the surfacetreatment procedure, its effects onadhesion, its relationship with thematerial’s composition, clinicalaspects, and expected longevitywere selected. Although not anexhaustive review, the conceptsincluded here were obtained fromthe surface treatment protocols lit-erature. Some illustrative clinicalsituations are presented as exam-ples of the suggested techniques.

TREATING CERAMIC

RESTORATIONS

The types of ceramic surface treat-ments and their correspondingcompositions are summarized inTable 1.

Mechanical TreatmentThe clinical success of ceramicrestorations seems to be dependenton the bonding quality developedover the entire prepared dentin.3,43

Composite cements present low sol-

ubility and good adhesion to thedental structure.44,45 These materi-als constitute a primary link whenconsidering the interaction betweenthe restoration and the tooth struc-ture. The micromechanical reten-tions to be created on the internalsurface of indirect restorations areessential to the process of bondingto the composite cement.1,3,7,33,46,47

Conventional dental porcelain is avitreous ceramic based on a silica

TABLE 1. CERAMICS COMPOSITION AND SURFACE TREATMENT PROTOCOLS.

Restorative Material Composition* Surface Treatment Protocols

Feldspar ceramics: Noritake EX3 SiO2; K2O, Al2O3, 6SiO2; 9.5% hydrofluoric acid for 2 to 2.5 min;(Noritake, Nagoya, Japan), Na2O, Al2O3, 6SiO2 application 1 min washing; silaneDuceram (Degussa Dental/Dentsply, Hanau, Germany)

Leucite-reinforced ceramics: SiO2, Al2O3 , K2O, Na2O, CeO2, 9.5% hydrofluoric acid for 60 s; IPS Empress, Cergogold other oxides 1 min washing; silane application

Lithium di-silicate–reinforced SiO2 (57–80%), Li2O (11–19%), 9.5% hydrofluoridric acid for 20 s;ceramic: IPS Empress II Al2O3 (0–5%), La2O3 (0.1–6%), 1 min washing; silane application

MgO (0–5%), P2O5 (0–11%), ZnO (0–8%), K2O (0–13%)

Glass-infiltrated aluminum oxide Al2O3 (82%), La2O3 (12%), Sandblasting: synthetic diamond particlesceramic: In-Ceram alumina SiO2 (4.5%), CaO (0.8%), (first choice) or 50 µm Al2O3 particles;

other oxides (0.7%) restoration by washing with water for 1 min; or retentive preparation design

Cements: phosphate-monomer-containing resincement (first choice), conventional resin cement, glass ionomer, or zinc phosphate

Zirconium-reinforced ceramic: Al2O3 (62%), ZrO2 (20%), Retentive preparation design; alternative:In-Ceram zirconium La2O3 (12%), SiO2 (4.5%), sandblasting with 50 µm Al2O3 particles

CaO (0.8%), other oxides (0.7%) Cements: phosphate-monomer-containing resin cement (first choice), conventional resincement, glass ionomer, or zinc phosphate

Densely sintered, aluminum Al2o3 (99.5%) Retentive preparation design; alternative:oxide ceramic: Procera AllCeram sandblasting with 50 µm Al2O3 particles

Cements: phosphate-monomer-containing resincement (first choice), conventional resin cement, glass ionomer, or zinc phosphate

*According to manufacturers.

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(SiO2) network and potash feldspar(K2O, Al2O3, 6SiO2) or sodafeldspar (Na2O, Al2O3, 6SiO2), oreven both components. In spite ofits esthetic qualities and high com-patibility to metal alloys, the felds-pathic ceramics are not resistant to tension and shear, presentingserious limitations to their beingemployed as metal-free restorativematerials.2,3,4,14,48–50

For the feldspathic ceramics, thechemical etching time should befrom 2 to 2.5 minutes with hydro-fluoric acid in a concentration vary-ing between 8 and 10%,46,51 whichpromotes a morphologic change ofthe ceramic surface, creating ahoneycomb-like topography, idealfor micromechanical bonding.1,51–53

This process is generated by the pref-erential chemical reaction betweenhydrofluoric acid and the silica phaseof feldspathic ceramics (6H2F2 +6SiO2 → 2H2SiF6 + 4H2O),54 thusforming a salt named hexafluorosili-cate, which is removed by waterspray.23,52–56 According to Della Bonaand colleagues, the bond strengthof composite cements increaseswith increasing ceramic surfaceroughness caused by acid-etching.22

Ceramics reinforced withleucite,3,12,18,19 lithium di-sili-cate,1,3,20–23 alumina, and zirco-nium3,12,14,15,24–26 have been largelyused as restorative materials, andthe surface treatment has been con-sidered a factor directly related tothe clinical success of those restora-

tions.1,3,12 Prior studies havedemonstrated positive results for IPSEmpress (Ivoclar-Vivadent, Schaan,Liechtenstein) and Cergogold(Degussa Dental/Dentsply, Hanau,Germany), which are examples ofleucite-reinforced ceramics, usinghydrofluoric acid for 60 sec-onds.1,20,38,39,57,58 An illustrativeclinical situation (Figures 1–6)depicts the substitution of unes-thetic amalgam restorations withleucite-reinforced ceramic onlays(Cergogold) surface treated withhydrofluoric acid.

The same process occurs in ceramicsreinforced with lithium di-silicate,such as the IPS Empress II system,which has a main crystalline phaseconstituted of long crystals embed-ded in a glassy matrix.20,59 The useof this system is demonstrated in anillustrative clinical situation (Fig-ures 7–10) of an anterior crownconstruction, surface-treated withhydrofluoric acid. According toDella Bona and colleagues, IPSEmpress I and II ceramic surfaceshave shown greater adhesion valueswhen conditioned by 9.5% hydro-fluoric acid compared with thevalue obtained with 4% acidulatedphosphate fluoride.38 Della Bonaand colleagues have also demon-strated that microstructural differ-ences between both systems haveled to the achievement of higheradhesion and flexure resistance val-ues for IPS Empress II. Borges andcolleagues related that 9.5% hydro-fluoric acid-etching for 20 seconds

is enough to remove the secondcrystalline phase and the glassymatrix, thus creating an adhesion-favorable surface.1 Airborne particleabrasion alone provides insufficientbond strengths.60,61 Excessive air-borne particle abrasion has inducedchipping or a high loss of ceramicmaterial and is therefore not recom-mended for cementing silica-basedall-ceramic restorations.12,61 Katoand colleagues compared airborneparticle abrasion with different acid-etching agents and found thathydrofluoric acid and sulfuric acid–hydrofluoric acid provided the highest and most durable bond strengths.53

However, hydrofluoric acid surfacetreatment promotes shallow surfacemicromechanical retentions in alu-minum oxide (Al2O3) or alumina-reinforced ceramic restorations due to its low silica content.1,3,13,26

In-Ceram alumina system (VitaZahnfabrik, Seefeld, Germany) has82% alumina, whereas the In-Ceramzirconium system (Vita Zahnfabrik)is reinforced with 62% alumina,20% zirconium oxide, and 12%lanthanum oxide.1 According toSen and colleagues, hydrofluoricacid chemical conditioning did notproduce good results for thoseceramics, and surface sandblastingcan be considered a good alterna-tive for creating a micromechanicaladhesion-favorable surface.40 Thisstudy also defined some importantparameters to be followed to maxi-mize the results of surface sand-

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Figure 1. Clinical situation 1. Occlusal view of Class IImesio-occluso-distal amalgam restorations in the upper rightsecond premolar and first molar.

Figure 2. Clinical situation 1.Occlusal view of onlay prepa-rations with palatine cusp coverage.

Figure 5. Clinical situation 1. Cementation of the restorationusing a dual-composite cement.

Figure 6. Clinical situation 1. Final clinical aspect obtainedwith a ceramic restoration.

Figure 3. Clinical situation 1. Surface treatment with9.5% hydrofluoric acid for 60 seconds

Figure 4. Clinical situation 1. Surface chemical treat-ment through the application of monocomponentsilane bonding agent for 1 minute.

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blasting: pressure to be applied,particle size, particle shape, inci-dence angle of the particle, and wetversus dry particles. As an alternativetreatment, silica coating and silaneapplication with the Rocatec System(3M ESPE Dental Products, St. Paul,MN, USA) seems to provide adurable resin bond to glass-infiltratedaluminum oxide ceramic withbisphenol A glycidyl methacrylate(BIS-GMA) composite cements.62–64

Awliya and colleagues and Kernand Thompson found significantlypositive results with the adhesion ofthe composite cement when submit-ting In-Ceram alumina, In-Ceramzirconium, and Procera AllCeram(Nobel Biocare, Gothenburg, Sweden) ceramics to the shear testafter sandblasting with 50 µm alu-minum oxide particles comparedwith hydrofluoric acid chemicaletching, diamond abrasion plus

phosphoric acid, or control (notreatment).3,12 In spite of this fact,Borges and colleagues showed thatsandblasting with 50 µm Al2O3

particles was not effective in increas-ing irregularities on the surface ofthese ceramics, which could meanan unreliable surface treatment toimprove adhesion.1 Aluminumoxide particles and alumina havesimilar hardness, which tends tocause flattening of the alumina

Figure 7. Clinical situation 2. Discoloration of the upper leftcentral incisor, the initial clinical aspect.

Figure 8. Clinical situation 2. Surface treatment of the crownwith 9.5% hydrofluoric acid for 10 seconds.

Figure 9. Clinical situation 2. Surface chemical treatmentthrough the application of a monocomponent silane couplingagent for 1 minute.

Figure 10. Clinical situation 2. Final clinical aspect obtainedwith a ceramic restoration.

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cristals.1 Thus, an alternative, atleast for glass-infiltrated aluminumoxide ceramics (In-Ceram alumina)is to use 1 to 3 µm diameter dia-mond particles, which show higherhardness rates than alumina parti-cles found in the restoration.40

Regarding densely sintered alu-minum oxide ceramic (Procera AllCeram), Blatz and colleaguesstate that the small number of long-term in vitro studies on its bondstrength does not allow for clinicalrecommendations.65 According toBorges and colleagues, the retentionshould be reached with a retentivepreparation design.1 In this way, itseems that restorations manufac-tured with these materials can becemented using glass ionomercements or even zinc phosphatecements. To improve bond strength,chemical treatment can be used asan additional technique, as dis-cussed below.

Chemical Treatment Silane is a bifunctional moleculethat acts as a bonding agentbetween the inorganic particles ofceramics and the adhesive compos-ite resin matrix.42,48,66,67 This bond-ing agent has a general chemicalstructure, R'—Si(OR)3, where R' isthe organofunctional group, typi-cally a methacrylate, that reacts tothe adhesive system or the compos-ite cement, creating a covalent bondafter polymerization.48,57 The alkylgroup (R) is hydrolyzed to a silanol(SiOH), creating a covalent bondwith the silicon inorganic particles

(Si—O—Si), completing the bond-ing process.48,57,68,69 According toPeumans and colleagues, silane hasfunctional groups that promotechemical bonding with hydrolyzedsilicon oxide from the ceramic sur-face, and with the methacrylategroup from the adhesive system orthe composite cement by copolymer-ization.46 Monocomponent systemsthat contain alcohol or acetone-diluted silane require hydrofluoricacid treatment of the ceramic sur-face so that the surface becomeschemically active. The same processis necessary for double-componentsolutions, in which silane is dilutedin an acid hydrous solution,hydrolyzing the coupling agent,which becomes able to react directlywith the ceramic surface. If notused for the right length of time,polymerization over silane willform nonreactive polysiloxanebonding chains.70

The application of a silane couplingagent (see Figures 4 and 9) is impor-tant to the adhesion of ceramicrestorations, which is responsiblefor the chemical union between theinorganic ceramic phase and theorganic phase of the compositecement.36,42,52,71–73 Della Bona andcolleagues have demonstrated anincrease in adhesive resistance whenusing silane with ceramics reinforcedwith feldspar, leucite, or lithium di-silicate, also concluding that onlythe application of silane over non-treated ceramics presents a low-resistant adhesive interface.38

Some studies have demonstratedsignificant results when associatingsilanization process with heat appli-cation, which helps to eliminatewater, alcohol, and other solvents,and thus promotes the condensa-tion reaction and the silica-silanecovalent bonding.74,75 Hooshmandand colleagues concluded that a15-second washing using 80°Cwater prior to a 30-second dryingusing a 50°C air jet promotes areduction of the number of adhe-sive flaws,75 which has also beenobserved by Roulet and colleagueswho used a 20°C temperature for60 seconds and 100°C for another60 seconds, obtaining a restorationadhesion twice as resistant com-pared with surface treatment without heat application.74

However, silane efficiency is com-promised in ceramic systems highlyreinforced with alumina becausethere is a reduced and unstableadhesion between silane and alu-mina.3,40 In addition, the silanechemical bonding reaction dependson the presence of silica on theceramic surface, which is not com-mon in the composition of aluminumceramics.3,40 An alternative is to usephosphate-monomer-containingcomposite cements, which seem toprovide strong and long-termdurable resin bonds to air particle–abraded, glass-infiltrated aluminumoxide ceramics and to glass-infiltratedzirconium oxide ceramics.62–65 Theadhesive functional phosphatemonomer 10-methacryloyloxyde-

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cyldihydrogen phosphate bondschemically to metal oxides such asaluminum and zirconium oxides.63

Some authors recommend the use of these cements without a silane or bonding agent,62 whereas otherssuggest a silane coupling agent toincrease wettability of the ceramicsubstrate.16,64 The use of a retentivepreparation design is indicated toobtain greater retention of alumina-reinforced ceramic systems, accord-ing to Borges and colleagues.1

TREATING INDIRECT COMPOSITE

RESIN RESTORATIONS

All types of laboratory-processedcomposite restorations, surfacetreatments, and their correspondingcompositions are summarized inTable 2.

The combination of polymerizationprocesses based on high light inten-sity, temperature, pressure, vacuum,and nitrogen atmosphere haveresulted in laboratory-processedcomposite resins reaching polymer-

ization levels of up to 80%,76

thus enhancing their mechanicalproperties and widening their indi-cations.77 Soares and colleagues,through a microtensile bond strengthtest, compared Targis and Solidex(Shofu Inc., Kyoto, Japan) indirectcomposite resins with Filtek Z250universal composite resin (3MESPE).33 They used laboratorypolymerization, hydrofluoric acidsurface treatment, and aluminumoxide particle sandblasting, andconcluded that no differences wereobserved between the laboratory-processed composite resin and thedirect composite resin in bondingwith the composite cement due tothe similarity in their compositions.

Surface treatment of laboratory-processed composite resin restora-tions with hydrofluoric acidpromotes a microstructural alter-ation of the composite because ofthe dissolution of the inorganic particles present in microhybridcomposites.78–81 However, surface

mechanical treatment in laboratory-processed composites using sand-blasting with aluminum oxideparticles seems to be the best alter-native to raise restoration surfaceenergy because it promotes a non-selective degradation of the resinand results in a better adhesion tothe composite cement.33,36,56,79,82

An illustrative clinical situation(Figures 11–15) demonstrates theconstruction of a Targis/Vectris(Ivoclar-Vivadent) glass fiber–reinforced composite fixed partialdenture; the composite resin of this system is classified as a second-generation resin with 67% inorganicparticles (by weight) and 33% BIS-GMA, decane dimethacrylate andurethane dimethacrylate organicmatrix.27 This case illustrates resinsandblasting with aluminum oxideparticles, showing the microscopi-cal characterization of the surface.

The presence of inorganic particleson the laboratory-processed com-posite resin surface makes it possi-

TABLE 2. LABORATORY-PROCESSED COMPOSITE COMPOSITION AND SURFACE TREATMENT PROTOCOLS.

Restorative Materials Composition* Surface Treatment Protocols

Solidex 61% UDMA and photostarters, Sandblasting:39% (vol) inorganic particles aluminum oxide for 10 s

Silane application

Targis 33% BIS-GMA, DMA, and UDMA; 67% (volume) inorganic particles

Artglass 30% methacrylates, 70% inorganic particles

belleGlass 26% UDMA and DMA; 74% inorganic particles

Filtek Z250 40% UDMA, BIS-EMA, BIS-GMA; 60% inorganic particles

BIS-GMA = bisphenol A glycidyl methacrylate; BIS-EMA = bisphenol-A polyethylene glycol diether dimethacrylate; DDMA = decane dimethacry-late; UDMA = urethane dimethacrylate.

*According to manufacturers.

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Figure 11. Clinical situation 3. Missing second right upperpremolar

Figure 12. Clinical situation 3. Surface sandblasting of aglass fiber–reinforced composite fixed partial denture with50 µm Al2O3 for 10 seconds.

Figure 13. Clinical situation 3. Scanning electron micro-scopic image of the Targis surface treated with aluminumoxide sandblasting, showing angular and irregular surface fis-sures; the silane coupling agent and the adhesive system willpenetrate these fissures (×1,000 original magnification).

Figure 15. Clinical situation 3. Final aspect obtained with aglass fiber–reinforced composite fixed partial denture.

Figure 14. Clinical situation 3. Internal surface chemicaltreatment through application of a monocomponent silanecoupling agent for 1 minute.

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ble to develop better adhesionthrough the application of a silanecoupling agent (see Figure 14).According to Soares and colleagues,aluminum oxide sandblasting didnot produce a significant increase inadhesive resistance, but when it wasassociated with silane, higher bondstrength values were obtained.33

Furthermore, the complete dissolu-tion of the inorganic particles pro-moted by hydrofluoric acid resultsin a surface characterized only by thepresence of resin organic matrix,1,52

which makes the restoration-to-cement adhesive interface less resis-tant.33 Since all laboratory-processedcomposite resins present similarcomposition, their surface treat-ment tends to be the same.33

CONCLUSIONS

Based on this literature review, itis possible to conclude that the sur-face treatment of ceramics and indi-rect composite resins depends onthe material composition, the use of abrading or etching techniques,and the employment of silanatingagents. Therefore, it is up to theclinician to acquire a thoroughknowledge of the restorative mate-rials and follow their specific proto-cols to optimize the success ofindirect restorative procedures.

DISCLOSURE

The authors do not have any finan-cial interest in the companies whosematerials are discussed in this article.

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Reprint requests: Carlos José Soares, DDS,MS, PhD, Faculdade de Odontologia—Universidade Federal de Uberlândia, Departamento de Dentística Restauradora,Av. Pará, n 1720, Campus Umuarama,Bloco 2B, Sala 2B-24,CEP 38405-902,Uberlândia, Minas Gerais, Brasil; e-mail:carlosjsoares@umuarama.ufu.br©2005 BC Decker Inc